KR100791731B1 - 자성체 코어 - 세라믹 쉘 나노 결정 및 그의 제조방법 - Google Patents
자성체 코어 - 세라믹 쉘 나노 결정 및 그의 제조방법 Download PDFInfo
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- KR100791731B1 KR100791731B1 KR1020070000997A KR20070000997A KR100791731B1 KR 100791731 B1 KR100791731 B1 KR 100791731B1 KR 1020070000997 A KR1020070000997 A KR 1020070000997A KR 20070000997 A KR20070000997 A KR 20070000997A KR 100791731 B1 KR100791731 B1 KR 100791731B1
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- 239000002159 nanocrystal Substances 0.000 title claims abstract description 74
- 239000000919 ceramic Substances 0.000 title claims abstract description 54
- 238000004519 manufacturing process Methods 0.000 title claims description 17
- 239000011162 core material Substances 0.000 claims abstract description 74
- 239000011257 shell material Substances 0.000 claims abstract description 51
- 239000002243 precursor Substances 0.000 claims abstract description 46
- 238000000034 method Methods 0.000 claims abstract description 28
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims description 50
- 239000011575 calcium Substances 0.000 claims description 45
- 239000011258 core-shell material Substances 0.000 claims description 38
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 12
- 239000002131 composite material Substances 0.000 claims description 11
- 238000000576 coating method Methods 0.000 claims description 8
- 238000010924 continuous production Methods 0.000 claims description 8
- 239000004094 surface-active agent Substances 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 7
- NKJOXAZJBOMXID-UHFFFAOYSA-N 1,1'-Oxybisoctane Chemical compound CCCCCCCCOCCCCCCCC NKJOXAZJBOMXID-UHFFFAOYSA-N 0.000 claims description 5
- 239000001506 calcium phosphate Substances 0.000 claims description 5
- 229910000389 calcium phosphate Inorganic materials 0.000 claims description 5
- CUJRVFIICFDLGR-UHFFFAOYSA-N acetylacetonate Chemical compound CC(=O)[CH-]C(C)=O CUJRVFIICFDLGR-UHFFFAOYSA-N 0.000 claims description 4
- 239000004254 Ammonium phosphate Substances 0.000 claims description 3
- 229920000463 Poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol) Polymers 0.000 claims description 3
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims description 3
- 235000019289 ammonium phosphates Nutrition 0.000 claims description 3
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 claims description 3
- 239000001639 calcium acetate Substances 0.000 claims description 3
- 229960005147 calcium acetate Drugs 0.000 claims description 3
- 235000011092 calcium acetate Nutrition 0.000 claims description 3
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 229920001400 block copolymer Polymers 0.000 claims 2
- 230000001376 precipitating effect Effects 0.000 claims 2
- 239000002105 nanoparticle Substances 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 54
- 230000002194 synthesizing effect Effects 0.000 description 9
- 239000007789 gas Substances 0.000 description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 230000000975 bioactive effect Effects 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 description 2
- BTOOAFQCTJZDRC-UHFFFAOYSA-N 1,2-hexadecanediol Chemical compound CCCCCCCCCCCCCCC(O)CO BTOOAFQCTJZDRC-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 210000000988 bone and bone Anatomy 0.000 description 2
- 235000011010 calcium phosphates Nutrition 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000012377 drug delivery Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 229920005862 polyol Polymers 0.000 description 2
- 150000003077 polyols Chemical class 0.000 description 2
- 239000011541 reaction mixture Substances 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 238000001890 transfection Methods 0.000 description 2
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 2
- 239000012692 Fe precursor Substances 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- SRYDOKOCKWANAE-UHFFFAOYSA-N hexadecane-1,1-diol Chemical compound CCCCCCCCCCCCCCCC(O)O SRYDOKOCKWANAE-UHFFFAOYSA-N 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000399 orthopedic effect Effects 0.000 description 1
- 125000000286 phenylethyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])C([H])([H])* 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- -1 polyethylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000001356 surgical procedure Methods 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- RMZAYIKUYWXQPB-UHFFFAOYSA-N trioctylphosphane Chemical compound CCCCCCCCP(CCCCCCCC)CCCCCCCC RMZAYIKUYWXQPB-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B26—HAND CUTTING TOOLS; CUTTING; SEVERING
- B26B—HAND-HELD CUTTING TOOLS NOT OTHERWISE PROVIDED FOR
- B26B27/00—Hand cutting tools not provided for in the preceding groups, e.g. finger rings for cutting string, devices for cutting by means of wires
- B26B27/007—Hand cutting tools not provided for in the preceding groups, e.g. finger rings for cutting string, devices for cutting by means of wires with handles specifically adapted to be attached to a human hand or finger, e.g. thimbles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y25/00—Nanomagnetism, e.g. magnetoimpedance, anisotropic magnetoresistance, giant magnetoresistance or tunneling magnetoresistance
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/0036—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties showing low dimensional magnetism, i.e. spin rearrangements due to a restriction of dimensions, e.g. showing giant magnetoresistivity
- H01F1/0045—Zero dimensional, e.g. nanoparticles, soft nanoparticles for medical/biological use
- H01F1/0054—Coated nanoparticles, e.g. nanoparticles coated with organic surfactant
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
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Abstract
Description
Claims (15)
- 연속공정으로 복합기능 자성체 코어-세라믹 쉘 나노 결정을 제조하는 방법에 있어서,자성체 코어 물질 전구체, 상기 코어 물질 전구체의 환원제를 혼합하는 단계;상기 자성체 코어물질 전구체와 상기 환원제의 용매를 혼합하여 제1 혼합용액을 형성하는 단계;상기 제1 혼합용액을 제1온도까지 가열하고, 제1시간동안 유지하는 단계;상기 제1 혼합 용액을 실온까지 냉각시켜 상기 자성체 코어 물질을 형성하는 단계;상기 자성체 코어물질에 세라믹 쉘 물질 전구체를 혼합하여 제2 혼합용액을 형성하는 단계;상기 제2 혼합용액을 제2온도까지 가열하고, 제2시간동안 유지하는 단계; 및상기 제2 혼합 용액을 실온까지 냉각시켜 상기 자성체 코어 물질에 상기 세라믹 쉘 물질을 코팅하는 단계를 포함하는 복합기능 자성체 코어-세라믹 쉘 나노결정 제조 방법.
- 제1항에 있어서,에탄올(ethanol)을 첨가하여 상기 복합기능 나노 결정을 석출하고 원심분리 기를 이용하여 분리하는 단계를 더 포함하는 것을 특징으로 하는 복합기능 자성체코어-세라믹 쉘 나노 결정 제조방법.
- 제1항에 있어서,상기 제1 혼합용액을 형성하는 단계에 계면활성제 첨가하는 단계를 추가적으로 가지는 것을 특징으로 하는 복합기능 자성체 코어-세라믹 쉘 나노 결정 제조방법.
- 제1항에 있어서,상기 제2혼합용액을 형성하는 단계에 계면활성제 첨가하는 단계를 추가적으로 갖지 않는 것을 특징으로 하는 복합기능 자성체 코어-세라믹 쉘 나노 결정 제조방법.
- 제1항에 있어서,상기 코어는 Fe3O4 이고, 상기 쉘은 Ca3(PO4)2 임을 특징으로 하는 자성체 코어 - 세라믹 쉘 나노 결정 제조방법.
- 제1항에 있어서,상기 제1 혼합용액을 상기 제1온도에서 일정시간 유지한 다음, 상기 제1온도 보다 높은 제3온도까지 가열하고 제3시간동안 유지하는 단계를 더 포함하는 것을 특징으로 하는 코어-쉘 나노 결정 제조방법.
- 제1항에 있어서,상기 제2 혼합용액을 상기 제2온도에서 일정시간 유지한 다음, 상기 제2온도보다 높은 제4온도까지 가열하고 제4시간동안 유지하는 단계를 더 포함하는 것을 특징으로 하는 코어-쉘 나노 결정 제조방법.
- 연속 공정으로 복합기능 마그네타이트-인산칼슘 코어-쉘 나노 결정을 제조하는 방법에 있어서,마그네타이트 전구체인 FeIII(acac)3 와 상기 마그네타이트 전구체의 환원제를 혼합하는 단계;용매인 디옥틸에테르 (dioctyl ether)를 혼합하여 제1 혼합용액을 형성하는 단계;상기 제1 혼합용액을 제300℃까지 가열하고, 1~2시간동안 유지하는 단계;상기 제1 혼합 용액을 실온까지 냉각시켜 상기 마그네타이트 코어를 형성하는 단계;상기 마그네타이트 코어에 칼슘 아세테이트(calcium acetate) 와 암모늄 포스페이트(ammonium phosphate) 및 이들의 환원제를 혼합하여 제2 혼합용액을 형성 하는 단계;상기 제2 혼합용액을 80℃까지 가열하고, 30분동안 유지하는 단계; 및상기 제2 혼합 용액을 실온까지 냉각시켜 상기 마그네타이트 코어에 상기 Ca3(PO4)2 쉘을 코팅하는 단계를 포함하는 복합기능 마그네타이트-Ca3(PO4)2 코어-쉘 나노 결정 제조 방법.
- 제8항에 있어서,에탄올(ethanol)을 첨가하여 상기 복합기능 나노 결정을 석출하고 원심분리기를 이용하여 분리하는 단계를 더 포함하는 것을 특징으로 하는 복합기능 마그네타이트-Ca3(PO4)2 코어-쉘 나노 결정 제조방법.
- 제8항에 있어서,상기 제1 혼합용액을 형성하는 단계에 계면활성제로 트리블록 코폴리머 (tri-block copolymer, PEO-PPO-PEO)를 첨가하는 단계를 추가적으로 가지는 것을 특징으로 하는 복합기능 마그네타이트-Ca3(PO4)2 코어-쉘 나노 결정 제조방법.
- 제8항에 있어서,상기 제2혼합용액을 형성하는 단계에 계면활성제 첨가하는 단계를 추가적으로 가지지 않는 것을 특징으로 하는 복합기능 마그네타이트-Ca3(PO4)2 코어-쉘 나노 결정 제조방법.
- 연속공정으로 복합기능 자성체 코어-세라믹 쉘 나노 결정을 제조하는 방법에 있어서,자성체 코어 물질 전구체, 상기 자성체 코어 물질 전구체의 환원제, 상기 코어물질 전구체와 상기 환원제의 용매를 혼합하여 제1 혼합용액을 형성하고, 가열 한 후, 냉각시켜 상기 자성체 코어 물질을 형성하는 단계; 및상기 자성체 코어물질 형성하는 동일한 장소에서 세라믹 쉘물질 전구체, 상기 세라믹 쉘물질 전구체의 환원제, 상기 세라믹 쉘물질 전구체를 혼합하여 제2 혼합용액을 형성하고, 가열한 후 냉각시켜 상기 자성체 코어 물질에 상기 세라믹 쉘물질을 코팅하는 단계를 포함하는 복합기능 자성체 코어-세라믹 쉘 나노 결정 제조 방법.
- 자성체 코어 물질 전구체, 상기 코어 물질 전구체의 환원제를 혼합하는 단계;상기 자성체 코어물질 전구체와 상기 환원제의 용매를 혼합하여 제1 혼합용액을 형성하는 단계;상기 제1 혼합용액을 제1온도까지 가열하고, 제1시간동안 유지하는 단계;상기 제1 혼합 용액을 실온까지 냉각시켜 상기 자성체 코어 물질을 형성하는 단계;상기 자성체 코어물질에 세라믹 쉘 물질 전구체와 상기 세라믹 쉘 물질 전구체의 환원제를 혼합하는 단계;상기 세라믹 쉘 물질 전구체를 혼합하여 제2 혼합용액을 형성하는 단계;상기 제2 혼합용액을 제2온도까지 가열하고, 제2시간동안 유지하는 단계; 및상기 제2 혼합 용액을 실온까지 냉각시켜 상기 자성체 코어 물질에 상기 세라믹 쉘 물질을 코팅하는 단계를 포함하는 연속공정으로 제조한 복합기능 자성체 코어-세라믹 쉘 나노 결정.
- 마그네타이트 전구체인 FeIII(acac)3 와 상기 마그네타이트 전구체의 환원제를 혼합하는 단계;용매인 디옥틸에테르 (dioctyl ether)를 혼합하여 제1 혼합용액을 형성하는 단계;상기 제1 혼합용액을 제60~80℃까지 가열하고, 1~2시간동안 유지하는 단계;상기 제1 혼합 용액을 실온까지 냉각시켜 상기 마그네타이트 코어를 형성하는 단계;상기 마그네타이트 코어에 칼슘 아세테이트(calcium acetate)와 암모늄 포스페이트(ammonium phosphate) 및 이들의 환원제를 혼합하여 제2 혼합 용액을 형성하는 단계;상기 제2 혼합용액을 80℃까지 가열하고, 30분 동안 유지하는 단계상기 제2 혼합 용액을 실온까지 냉각시켜 상기 마그네타이트 코어에 상기 Ca3(PO4)2 쉘을 코팅하는 단계를 포함하는 연속 공정으로 제조한 복합기능 마그네타이트-Ca3(PO4)2 코어-쉘 나노결정.
- 자성체 코어 물질 전구체, 상기 자성체 코어 물질 전구체의 환원제, 상기 코어 물질 전구체와 상기 환원제의 용매를 혼합하여 제1 혼합용액을 형성하고, 가열 한 후, 냉각시켜 상기 자성체 코어 물질을 형성하는 단계; 및상기 자성체 코어 물질 형성하는 동일한 장소에서 세라믹 쉘 물질 전구체, 상기 세라믹 쉘 물질 전구체의 환원제, 상기 세라믹 쉘 물질 전구체를 혼합하여 제2 혼합용액을 형성하고, 가열한 후 냉각시켜 상기 자성체 코어 물질에 상기 세라믹 쉘 물질을 코팅하는 단계를 포함하는 연속공정으로 제조한 복합기능 자성체 코어-세라믹 쉘 나노결정.
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